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Hydroxyapatite, Synthesis of Numerous Cds Quantum Dot Composite

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 International Journal of
Nanomaterials and Nanostructure
eISSN: 2455-5584 (Online)
Vol. 5: Issue 1
www.journalspub.com

Hydroxyapatite, Synthesis of Numerous Cds Quantum Dot

Composite Material: A Review
Binoy Bera
Department of Computer Science and Engineering, West Bengal University of Technology,
Kolkata, West Bengal, India

ABSTRACT
Hydroxyapatite is one of most interesting material which is used as chemical sensor for
detecting different hazardous gases. It is a bio-ceramic and non-toxic material for which it is
widely used in bioengineering. On the other side, CdS quantum dot is very important material
in optoelectronic device fabrication for its fascinating optical, physical and electronic
properties. Furthermore, scientists are also doing their research very widely on CdS quantum
dot for their better fluorescence and optical properties. Here in this paper, synthesis
procedure of different composite material with CdS quantum dot has been reviewed. A brief
review about hydroxyapatite and its application were also described. Different procedure for
synthesis of hydroxyapatite material has also been reviewed.

Keywords: Hydroxyapatite, gas sensor, biocompatibility, CdS quantum dot, MoS2, Porous
silicon, Polyvinylidene fluoride.

*Corresponding Author
E-mail: berabinoy17@gmail.com

INTRODUCTION (PPy) [9] and polythiophene (PT) [10] are

Recently the technologies are developing
day by day which is also somehow become
responsible for some environment
problems such as air pollution, industrial
pollution etc. Especially carbon-based gas
like carbon di-oxide, carbon monoxide and
other hazardous gases are very dangerous
for human health. So, it is necessary to
detect such fatal gases for public safety.
Several materials like ZnO [1], SnO2 [2],
TiO2 [3], CuO [4], WO3 [5], Cr2O3 [6] and
In2O3 [7] have been used to develop
sensors for detecting such gases. However,
the operating temperature of all these
material-based gas sensors is above 300°C.
Furthermore, some composite material
fabricated with conductive polymer such
as polyaniline (PAni) [8], polypyrrole
used to design such sensors for their good
physical and chemical properties.
composite materials such as PPy/WO3
[11], PPy/SnO2 [12], PPy/ZnO [13],
PPy/Fe2O3 [14], PPy/MoO3 [15], PPy/NiO
[16], PAni/SnO2 [17] and PAni/TiO2 [18]
has already been used for detecting H2S,
NH3 and NO2. But there is still a
challenging issue for developing new kind
of chemical sensors which would show
good sensitivity, response/recovery time,
selectivity. On the other hand,
Hydroxyapatite [Ca10(PO4)6(OH)2;
abbreviated as HAp] is a bioceramic
material is used in bone and tissue
engineering because of its chemical
similarity to natural bone and excellent
biocompatibility. It has a hexagonal

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Hydroxyapatite, Synthesis of Numerous Cds Quantum
structure and a stoichiometric Ca/P ratio of
1.67, which is identical to bone apatite.
Furthermore, it has application in several
fields like catalyst [19], ion exchanger
[20], electrolyte for high temperature fuel
cell [21], protein separation [22], and
biosensors [23]. Specially nano-HAP is
used in Bone tissue engineering, Bone
void fillers for orthopaedic, traumatology,
spine, maxillofacial and dental surgery,
orthopedic and dental implant coating,
restoration of periodontal defects,
edentulous ridge augmentation endodontic
treatment like pulp capping, Repair of
mechanical furcation perforations and
apical barrier formation, Fillers for
reinforcing restorative glass ionomer
cement (GIC) and restorative composite
resin, Desensitizing a gentinpost teeth
bleaching, Remineralizing agent in
toothpastes, Early carious lesions
treatment, Drug and gene delivery.
Recently, it has got attention for
developing gas sensor for large surface P-
OH groups present in it which is the
reason for its interaction with gases. The
hydroxyapatite crystal composed of
(PO4)3+, OH-, and Ca2+ which possesses
exchange ion capacity with gas molecule.
For synthesis of HAP bioceramic material,
several methods like sol–gel [24],
hydrothermal processing [25], microwave
route [26], ultrasonic spray pyrolysis way
[27], precipitation route [28], emulsion
system [29] and sonochemical synthesis
[30] have been discovered. On the other
hand, In nanotechnology, quantum dot are
most promising material due to their
extraordinary optical [31], physical [32]
and electronic properties [33]. The
diameter range of such quantum dot are
from 2 to 10 nm. It’s a semiconductor-
based nano-sized material consists from
the II-VI and III-V periodic group
elements. Specially the electronic and
optical properties are quite interesting due
to the quantum confinement effect of
electrons and holes. Absorption and
IJNN (2019) 1-11 © JournalsPub 2019. All Rights Reserved
Binoy Bera
emission property of such quantum dot can
be tuned by varying its particle size. Due
to their luminescence properties, it is
extensively used in biological field such as
targeting drug delivery. Among all
quantum dots, CdS is very well-known
studied material for their direct band gap
of 2.4 eV. It has several applications in
biological field, photovoltaic cells, light
emitting diodes. However, for synthesis of
quantum dot, several methods including
hot injection, solvothermal, hydrothermal,
hydrogel, microwave, electrochemical and
reverse micelle have been discovered.
Beside these, since the discovery of
graphene, a two-dimension material, single
layer MoS2 is most interesting for their
ecstatic applications in solar cells,
wearable devices, catalysis, double-layer
capacitors, lubricants, photo emitting
devices etc. It is direct band gap (1.9 eV)
material whereas bulk MoS2 [34-44] is a
indirect band gap (1.2 eV) material. It has
good electronic, optical and physical
properties for its quantum and surface
effects. Furthermore, numerous methods
such as liquid/chemical exfoliation,
electrochemical exfoliation, hydrothermal
method, chemical vapor deposition,
mechanically exfoliation etc have been
discovered for preparation of MoS2
nanosheets. Again, Porous silicon [45-48]
is an important and extensively studied
material in the field of medical and drug
delivery due to its biocompatible,
biodegradable and nontoxic properties. It
is a silicon-based material with
interconnecting porous structure.
However, silicon is an indirect band gap
material which is not suitable in many
areas specially in optoelectronics device
applications [49-53]. Though silicon has
applications in several optoelectronic
devices such as photodetectors,
waveguides, solar cells but it is not
suitable for fabricating LED and LASER
for its indirect band gap. In that case
porous silicon with direct band gap is
Page 2
 International Journal of Nanomaterials and Nanostructure
much more interesting material for
manufacturing LED and LASER. But
there is still many challenges like stability
and efficiency, for developing such this
devices using porous silicon. Due to the
quantum confinement effect of porous
silicon, it can trap more light in silicon
cells. Depending on the pore size, it can be
classified in three categories such as
Microporous (pore size <5nm),
Mesoporous (pore size = 5 nm-50 nm) and
Macroporous (pore size >50nm).
Furthermore, polyvinylidene fluoride or
PVDF is a very well-known polymer
material for its piezoelectricity, flexibility
and non-toxicity. Depending on chain
Fig. 1: Properties of hydroxyapatite material.
MATERIAL AND METHODS
Hydroxyapatite Synthesis
Sol-Gel Process
The method involves the dilutions of
triethyl phosphite in anhydrous ethanol
and a small amount of distilled water for
hydrolysis. Once the hydrolysis is
completed (signified by a transformation
of an opaque solution to transparent), a
stoichiometric amount of calcium nitrate,
dissolved in anhydrous ethanol, is added
drop-wise with continuous stirring. Further
stirring and subsequent oven drying results
in a white gel which is ground with a
mortar to a fine powder and heated in a
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conformation structure, it is classified in
four phases α, β, γ and δ. Among all these
β, γ are most important due to its
piezoelectric activity. Here in this paper,
a little concept about the synthesis
method of HAP material has been
reviewed and a little application on gas
sensor were also provided. A review
about the synthesis procedure of different
composite material of CdS quantum dot
such as CdS quantum dot thin film grown
on MoS2 nanosheets decorated PVDF film,
CdS quantum dot embedded Porous
Silicon, CdS quantum dot – MoS2
nanosheets has also been described.
furnace (for 2 hours) at various
temperatures. Some polymer and
nanomaterial [54-62] is also synthesized
through this process.
Hydrothermal Processing
Sodium tripolyphosphate (Na5P3O10,
STTP), CaCl2, and urea ((NH2)2CO) were
of analytical grade (Sinopharm Chemical
Reagent Co., Ltd.). L-Glutamic acid (Glu)
was of biochemical grade (Huashun
Biochemical Reagent Co., Ltd.). All
reagents were used as received without
further purification.
Page 3
Hydroxyapatite, Synthesis of Numerous Cds Quantum Binoy Bera

In a typical synthesis, CaCl2 (0.0555 g, 0.5
mmol) was dissolved in 20 mL of
deionized water, Glu (0.2943 g, 2 mmol)
was added and dissolved in CaCl2 solution
under magnetic stirring with a slight
heating. STTP (0.0368 g, 0.1 mmol) was
dissolved in another 20 mL of deionized
water under magnetic stirring; urea
(0.1502 g, 2.5 mmol) was added and
dissolved in TPP solution. Then, the
solution containing CaCl2 and Glu was
added dropwise into the solution
containing TPP and urea under magnetic
stirring. After 30 min of stirring, the
mixture was transferred to and sealed in a
50 mL teflon-lined stainless-steel
autoclave and heated to 180 °C for 10 h
and then cooled to room temperature. The
precipitate was collected and washed
alternately with ethanol and deionized
water by centrifugation (9000 rpm, 5 min),
and then dried at 60 °C in the air. The pH
values of the mixture before and after the
synthesis reaction were measured by a pH
meter. In a series of syntheses, the
different molar ratios of reactants were
adjusted as listed in Table 1.
kept inside the domestic microwave oven
(Batliboy, Eddy: Operating at 2.45 GHz
and with a variable power up to a
maximum of 980 W). The solution mixture
was microwave irradiated for about 20-25
min, keeping the rate of boiling from
going beyond control. Since the ambient in
the oven was considered a factor in the
course of the reaction, the irradiation was
performed both in air and in ultra-pure
nitrogen (to avoid contact with
atmospheric CO2). Water was boiled out in
about 20 min and a dry looking product
remained in the flask.
Ultrasonic Spray Pyrolysis Way
A Ca(OOCCH3)2 solution (Merck) and
(NH4)2HPO4 (Merck) with a molar ratio
Ca/P equal to 1.67 was dissolved in
distilled water to obtain a total
concentration of 0.5 M. The solution was
atomized to generate droplets using an
ultrasonic nebulizer (1.7 MHZ, NE-U17,
Omron). The average diameter of the
droplets from the ultrasonic nebulizer was
4.3 µm based on Lang’s equation [16], as
follows:

Table 1. Co ncentra tiq n Of Reagents Ued D=0.34 (8πγ/ρf2)1/3 …………… (1)

For the Syn thesis of Ha
no. CaCl2a 1 STTP Glu urea where γ is the surface tension of the
sob 25 25 0 625 solution (N/m), ρ is the density of the
Sl 125 25 250 625 solution (kg/m3), and f is the frequency of
S2 125 25 500 625 the nebulizer (Hz). Nitrogen was used as
53 12.5 2.5 50 62.5 the carrier gas with a flow rate of 1 L/min
PO 125 250 0 625 to carry droplets to the heated tubular
Pl 125 250 250 625
P2 125 25 500 625 furnace. The droplet number concentration
P3 12.5 25 50 62.5 was estimated to be approximately
a
The unit of the concentrations is mmol/L. bLetter S 1012/m3 based on the volume of the
in the sample names means Ca/P ratio of the reagent is at precursor solution that was atomized by
stoichiometry of HA (1.67). Letter P in the names means the the carrier gas with a flow rate of 1 L/min.
concentration of phosphate is 10 times higher (Ca/P equals 0.167).
The tubular furnace consisted of a ceramic
tube with an inside diameter of 1.8 mm
Microwave Route and a length of 300 mm equipped with a
In the present procedure, equivolumes of temperature controller in order to maintain
0.24 M (NH4)2 HPO4 solution and 0.4 M the furnace temperature. The furnace was
aqueous suspension of Ca(OH)2 are mixed isothermally heated through the furnace
together (total volume of 150-250 cc), wall at 500, 700, 900, and 1000 °C. An
taken in a flat bottomed glass flask and electrostatic precipitator was used to

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 International Journal of Nanomaterials and Nanostructure
collect particles and was maintained at
150°C to hinder water condensation.
Precipitation Route
Calcium nitrate tetra hydrate
(Ca(NO3)2.4H2O), di-ammonium
hydrogen phosphate ((NH4)2HPO4) and
ammonia solution were used to synthesis
HAP nano particle, these analytical grade
chemicals are purchased from Merck used
without any further purification. 1M of
calcium nitrate and 0.6M of di-ammonium
hydrogen phosphate dissolved in double
distilled water in room temperature.
Phosphate solution was added with drop
by drop in calcium nitrate solution at
temperature 75°C and pH was maintained
at 11 for throughout the experiment using
ammonia solution. The resultant sol-gel
was continuously stirred at a temperature
75°C for 12 h at a constant pH of 11 and
this product was allowed to cool for 24
hours and then aged gels washed with
double distilled water and ethanol at least
three times. Finally, sol-gel was kept in hot
air oven at 85°C for overnight.
Emulsion System
The chemicals used in this work include
CaCl2·2H2O, (NH4)2HPO4, iso-octane and
ammonia solution (25%) which were used
as a Ca2+ source, a PO4 3− source, a OH−
source and an organic membrane phase,
respectively. They were AR grade and
obtained from Merck. The biodegradable
nonionic surfactants, Span 20 and Tween
80, were supplied by Fluka. Fatty acid, n-
caproic acid was used as an extractant
(carboxylic acid extractor) was supplied by
Sigma.
An internal water phase of W/O emulsion
was 30 mL of 0.5 M (NH4)2HPO4 solution
solubilized in the organic membrane phase
at volume ratio of 3:4. The membrane
phase comprises iso-octane, n-caproic acid
(1.5 mL) and 5 g of surfactant mixture
(1:1) of Span20 and Tween80. They were
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emulsified mechanically by mixing with a
homogenizer at the rotation of 14,000 rpm
for 5 min. The obtained W/O emulsion
was added to an external water phase
containing 1.0 M CaCl2·2H2O (15–30 mL)
and 50 mL of 25% ammonia solution. The
total volume of external water phase
volume was controlled at constant volume
of 80 mL by adding deionized water.
Stirring at vigorously speed was required
to disperse W/O emulsion droplet to form
W/O/W emulsion. After stirring for 30
min, the W/O/W emulsion was left to
allow aging and separating the W/O
emulsion from external water phase. The
upper emulsion phase was washed with
deionized water, followed by
centrifugation (12,000 rpm 30 min at 25
◦C) to remove both residue external phase
and organic membrane phase. Then, the
solid particles were washed with ethanol
followed by centrifugation in order to
completely remove the organic membrane
phase. The particles obtained were finally
dried at 105 ◦C for 2 h. The effects of
initial Ca/P molar ratio (Ca/Pi), reaction
temperature and calcination temperature in
the range of 1.00–2.00, 30–80 and 450–
750 ◦C were studied, respectively
Sonochemical Synthesis
Chemical reagents selected for use in this
work were H3PO4 (Wako Chemicals, 85%
in assay) and Ca(OH)2 (Wako Chemicals).
The mean particle size and specific surface
area (SSA) of Ca(OH)2 used were 22.8 μm
and 20.7 m2/g, respectively. These samples
were weighed in molar ratio to coincide
the stoichiometric HAp (Ca/P: 1.67), and 5
g of the mixture was suspended in 100 ml
of distilled water in a vial. A tool for
irradiating ultrasound was an available
commercial device (UT-600, ultrasonic
homogenizer, Nihonseiki Kaisha, Japan)
that produces acoustic wave at a frequency
of 20 kHz with a maximum power of 600
W. The sonic horn made of Ti (tip
Page 5
Hydroxyapatite, Synthesis of Numerous Cds Quantum
diameter×length=φ12mm×60mm) was
driven by a PZT transducer, and it was
dipped into the suspension around 10 mm
apart from the bottom of the vial. The
suspension was subjected to irradiation of
ultrasound at the optimum sonicating
conditions. The sonicating power and
amplitude were adjusted to provide
maximum power output of the generator.
The periods of irradiating time were set
from 5 to 120 min. During the ultrasonic
treatment for desired time, temperature
and equilibrium pH of the suspension were
monitored continuously. It was noted that
the temperature of the suspensions was
varied from 42∘C to 65∘C regarding the
irradiating time. The suspension was then
centrifuged and washed with distilled
water; subsequently, the solid phase
(powder) was dried at 65∘C for 24 h. In
order to confirm the sonochemical
reliability, heating the suspension was also
undertaken to determine the formation of
HAp under the same conditions as those of
ultrasonic irradiation. Heating treatment
was carried out at the same temperature
range from 42∘C to 65∘C as that in the
sonicating treatment according to the
length of time.
MoS2 Nanosheets
For synthesis of MoS2 nanosheets,
hexaammonium heptamolybdate
tetrahydrate and thiourea is used as main
material. First 1.24 g of hexaammonium
heptamolybdate tetrahydrate and 2.28 g of
thiourea is dissolved in 36ml deionized
water under vigorous stirring for a definite
time to form a homogeneous solution.
Then this solution are transferred to a 50
ml teflon lined stainless steel autoclave
and placed a cupper plate onto this
autoclave with a fixed angle. After that,
cupper plate containing solutions were
kept in a hot air oven with 2000C for 24
hrs. finally the samples is washed with di-
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Binoy Bera
water, ethanol respectively and dried with
temperature of 60°C.
MoS2 Nanosheets -CdS Quantum Dot
On the other hand, for synthesis of CdS
quantum dot, The cationic precursor 0.1 M
of Cadmium nitrate (Cd(NO3)2.4H2O) is
dissolved in 20 ml of ethanol (C2H6O)
solution. Then, the anionic precursor 0.1
M of thiourea (CH4N2S) is dissolved in
the same solution.\
The MoS2 nanosheets coated cupper plate
is immersed in the prepared solution for 1
minute. Finally, the samples are dried in
hot air oven for few minutes.
Porous Silicon-CdS Quantum Dot
Composite
Porous silicon samples is prepared from
single crystalline p-type<100> Si wafers.
These is first cleaned in a solution of 1:1:5
NH4OH:H2O2:H2O for 10 min at 70-80
ºC, then in 1:50 HF:H2O for 15 sec and
finally in 1:1:6 HCL:H2O2:H2O for 10
min at 70-80 0C. Porous silicon is made by
vapour phase strain etch process. The ratio
of hydrofluoric acid and nitric acid that is
used in our laboratory is 8:1. Here zinc
dust is used as sacrificial metal. After that,
porous silicon is immersed in the CdS
quantum dot containing solution.
Cds Quantum Dot Thin Film Grown On
MoS2 Nanosheets Decorated PVDF Film
For synthesis of that sample MoS2
nanosheets decorated PVDF film is
immersed in the CdS quantum dot
containing solutions.
APPLICATIONS OF
HYDROXYAPATITE
Hydroxyapatite is a major component and
an essential ingredient of normal bone and
teeth. Hydroxyapatite gives the bone and
teeth its rigidity. It is used to replace the
original affected teeth by artificial HAP
Page 6
 International Journal of Nanomaterials and Nanostructure
made teeth. Nanoporous [63-66]
hydroxyapatite is also used to deliver
drugs in human body. Researchers already
developed CNT doped nano-HAp thick
film for gas sensing application. Different
types of hazardous gases such as carbon
Fig. 2: Applications of hydroxyapatite material.
CONCLUSIONS
CdS quantum dot composite can be used in
several optoelectronic applications. CdS
quantum dot can be used to enhanced the
electroactive phase of PVDF thin film.
Due to the outstanding properties of CdS
quantum dot, it can be used as additive in
several applications with other
nanomaterial. Due to its excellent optical
and electronic property, it is also used in
fabricating optoelectronic devices.
Hydroxyapatite is very much important for
gas sensor, bone and tissue engineering
applications.
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Cite this Article: Binoy Bera. Hydroxyapatite, Synthesis of numerous CdS
quantum dot composite material: A Review. International Journal of
Nanomaterials and Nanostructure. 2019; 5 (1) 1–11p
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